#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:44:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179075 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/37/4303791.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4303791
loop_
_publ_author_name
'Joshua L. Mertz'
'Nan Ding'
'Mercouri G. Kanatzidis'
_publ_section_title
;
Three-Dimensional Frameworks of Cubic (NH4)5Ga4SbS10,
(NH4)4Ga4SbS9(OH).H2O, and (NH4)3Ga4SbS9(OH2).2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10898
_journal_page_last               10900
_journal_paper_doi               10.1021/ic901927r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'Ga4 H20 N5 S10 Sb'
_chemical_formula_weight         811.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mercouri G. Kanatzidis'
_audit_contact_author_address
;
Department of Chemistry
Northwestern University
2145 North Sheridan Road
Evanston, IL 60208
USA

;
_audit_contact_author_email      m-kanatzidis@northwestern.edu
_audit_contact_author_fax        847-491-5937
_audit_contact_author_phone      847-467-1541
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-10-28 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9000(5)
_cell_length_b                   12.9000(5)
_cell_length_c                   12.9000(5)
_cell_measurement_reflns_used    33015
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.35
_cell_measurement_theta_min      5.47
_cell_volume                     2146.69(14)
_computing_cell_refinement       X-area
_computing_data_collection       X-area
_computing_data_reduction        X-area
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18526
_diffrn_reflns_theta_full        32.19
_diffrn_reflns_theta_max         32.19
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    7.165
_exptl_absorpt_correction_T_max  0.8817
_exptl_absorpt_correction_T_min  0.7176
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   XRED32
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.945
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.294
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.398
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         2453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.398
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0085P)²+45.1772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                2377
_reflns_number_total             2453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901927r_si_004.cif
_cod_data_source_block           02159d1214
_cod_database_code               4303791
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.63895(5) 0.36105(5) 0.86105(5) 0.01114(19) Uani 1 3 d S . .
Ga1 Ga 0.72152(9) 0.22188(9) 1.08382(9) 0.0138(2) Uani 1 1 d . . .
Ga2 Ga 0.65548(11) 0.15548(11) 1.34452(11) 0.0249(5) Uani 1 3 d S . .
S4 S 0.6873(2) 0.18436(19) 0.9130(2) 0.0155(4) Uani 1 1 d . . .
S5 S 0.6137(2) 0.1185(2) 1.1762(2) 0.0222(5) Uani 1 1 d . . .
S6 S 0.6872(2) 0.3936(2) 1.1075(2) 0.0165(5) Uani 1 1 d . . .
S7 S 0.5575(3) 0.0575(3) 1.4425(3) 0.0505(19) Uani 1 3 d S . .
N1 N 0.9486(8) 0.4486(8) 1.0514(8) 0.024(3) Uani 1 3 d S . .
N2 N 0.4438(10) 0.3176(13) 1.1597(11) 0.046(3) Uani 1 1 d . . .
N3 N 0.3680(16) 0.3680(16) 1.3680(16) 0.105(13) Uani 1 3 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.01114(19) 0.01114(19) 0.01114(19) 0.0009(2) -0.0009(2) -0.0009(2)
Ga1 0.0145(5) 0.0126(5) 0.0143(5) 0.0001(4) -0.0031(4) -0.0009(4)
Ga2 0.0249(5) 0.0249(5) 0.0249(5) -0.0031(5) -0.0031(5) 0.0031(5)
S4 0.0200(11) 0.0118(10) 0.0147(11) -0.0010(9) -0.0044(9) -0.0013(9)
S5 0.0198(12) 0.0240(13) 0.0227(13) 0.0014(10) -0.0014(10) -0.0074(9)
S6 0.0220(12) 0.0123(10) 0.0151(11) -0.0016(8) -0.0039(9) -0.0008(9)
S7 0.0505(19) 0.0505(19) 0.0505(19) 0.0117(17) 0.0117(17) -0.0117(17)
N1 0.024(3) 0.024(3) 0.024(3) 0.002(4) 0.002(4) -0.002(4)
N2 0.028(6) 0.066(9) 0.044(8) -0.009(7) -0.012(5) 0.000(6)
N3 0.105(13) 0.105(13) 0.105(13) -0.027(13) -0.027(13) -0.027(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Sb1 S4 94.98(9) 10_646 . ?
S4 Sb1 S4 94.98(9) 10_646 7_665 ?
S4 Sb1 S4 94.98(9) . 7_665 ?
S5 Ga1 S6 114.40(11) . 8_746 ?
S5 Ga1 S6 112.48(12) . . ?
S6 Ga1 S6 111.32(14) 8_746 . ?
S5 Ga1 S4 105.20(11) . . ?
S6 Ga1 S4 105.53(10) 8_746 . ?
S6 Ga1 S4 107.20(10) . . ?
S7 Ga2 S5 106.94(9) . 11_567 ?
S7 Ga2 S5 106.94(9) . 8_746 ?
S5 Ga2 S5 111.88(8) 11_567 8_746 ?
S7 Ga2 S5 106.94(9) . . ?
S5 Ga2 S5 111.88(8) 11_567 . ?
S5 Ga2 S5 111.88(8) 8_746 . ?
Ga1 S4 Sb1 96.60(10) . . ?
Ga1 S5 Ga2 103.39(13) . . ?
Ga1 S6 Ga1 102.50(11) 11_567 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 S4 2.457(3) 10_646 ?
Sb1 S4 2.457(3) . ?
Sb1 S4 2.457(3) 7_665 ?
Ga1 S5 2.266(3) . ?
Ga1 S6 2.269(3) 8_746 ?
Ga1 S6 2.280(3) . ?
Ga1 S4 2.299(3) . ?
Ga2 S7 2.190(8) . ?
Ga2 S5 2.288(3) 11_567 ?
Ga2 S5 2.288(3) 8_746 ?
Ga2 S5 2.288(3) . ?
S6 Ga1 2.269(3) 11_567 ?
